Microscale crystallization

These steps are illustrated in Figure 11.4. It should be pointed out that a microscale crystallization with a Craig tube involves the same four steps, although the apparatus and procedures are somewhat different (see Section 11.4). 

The four steps in a semimicroscale or microscale crystallization are summarized in Table 11.1. 

Craig Tube Crystallizations, The Craig tube is commonly used for microscale crystallizations in the range of 10-100 mg of material (Fig. 5.30). The process consists of the following steps. 

In summary, it is clear that the micromechanical shock response of single crystal LiF is extremely complex. These results certainly temper the initial enthusiasm associated with Taylor s [9] study of Armco iron as a eomplete explanation for the relationship between the microscale and the macroscale in shock-loaded solids. 

Chaudhari AM, Woudenberg TM, Albin M, Goodson KE (1998) Transient liquid crystal thermometry of microfabricated PCR vessel arrays. J Microelectromech Sys 7 345-355 Cheng P, Wu WY (2006) Mesoscale and microscale phase heat transfer. In Greene G, Cho Y, Hartnett J, Bar-Cohen A (eds) Advances in heat transfer, vol 39. Elsevier, Amsterdam Choi SB, Barron RF, Warrington RQ (1991) Fluid flow and heat transfer in micro- tubes. ASME DSC 40 89-93... 

For this method, either a weighed amount of the solute (or a definite amount of the solvent) is placed in a suitable vessel. While agitating the system at constant temperature, known amounts of the solvent (or the solute) are added gradually until the solubility limit is reached. Appropriate checks must be carried out to ensure that the system is very close to equilibrium when the content or temperature of the system is recorded. In this method of temperature variation, attention is usually focused on the last small crystal. The equilibrium temperature is taken as the mean of the two temperatures at which the crystal either slowly grows or slowly dissolves. This procedure may also be carried out at the microscale by examining a small volume of the system under a hot-stage microscope. 

The term meso will be used to describe local chain organizations that occur within the nano- and microscale regions (Figure 18.2). While the terms mesophase and mesoregions have been employed in describing order within liquid crystals, the definition will be... 

The first semi-high-throughput automated system to dispense crystallization trials of less than 1 jl1 was designed in 1990 to deliver batch trials imder oil (Chayen et ah, 1990). The method was named microbatch to define a microscale batch experiment. It was designed to obtain maximum information on the molecule to be crystallized while using minimal amounts of sample. In order to prevent the evaporation of such small volumes, the trials are dispensed and incubated under low density (0.87 g/cm ) paraffin oil (Fig. 3.2). The crystallization drops remain under the oil since the aqueous drops are denser than the paraffin oil. 

Connection between Transport Processes and Solid Microstructure. The formation of cellular and dendritic patterns in the microstructure of binary crystals grown by directional solidification results from interactions of the temperature and concentration fields with the shape of the melt-crystal interface. Tiller et al. (21) first described the mechanism for constitutional supercooling or the microscale instability of a planar melt-crystal interface toward the formation of cells and dendrites. They described a simple system with a constant-temperature gradient G (in Kelvins per centimeter) and a melt that moves only to account for the solidification rate Vg. If the bulk composition of solute is c0 and the solidification is at steady state, then the exponential diffusion layer forms in front of the interface. The elevated concentration (assuming k < 1) in this layer corresponds to the melt that solidifies at a lower temperature, which is given by the phase diagram (Figure 5) as... 

Crystallization, triggered by the addition of a miscible nonsolvent (antisolvent) to a solute-containing solvent system, can be used to produce microscale particles with narrow particle size distributions. The process is complex as it involves the coupling... 

The most unpredictable process in X-ray structure determination is the crystallization of the candidate protein into a form suitable for X-ray diffraction. Each protein requires a unique set of conditions to form crystals. Typically 100 mg of highly purified protein is required to determine the conditions that result in usable crystals of 0.1 to 0.3 mm size, although a size of 0.3 to 0.8 mm is preferred. The occurrence of crystals and the rate of crystallization are influenced by many factors such as protein purity, the solvent, concentration of added precipitants, pH, temperature, and the presence of ions and cofactors. The protein solution at a concentration of typically 5 to 20 mg/ml is allowed to slowly reach supersaturation by the removal of or by changing the composition of the solvent by liquid-liquid diffusion or vapor diffusion methods. Microscale methods have been developed to explore several crystallization conditions simultaneously using minimum amounts of the purified protein sample. Recently, use of the zero gravity atmosphere in space has been explored as a means of facilitating crystallization (Eisenberg and Hill, 1990 Branden and Tooze, 1991 Tomasselli et al, 1991). 

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